CN105566249B - Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine - Google Patents
Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine Download PDFInfo
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- CN105566249B CN105566249B CN201511004146.4A CN201511004146A CN105566249B CN 105566249 B CN105566249 B CN 105566249B CN 201511004146 A CN201511004146 A CN 201511004146A CN 105566249 B CN105566249 B CN 105566249B
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- bentazon
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- solid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
- C07D285/15—Six-membered rings
- C07D285/16—Thiadiazines; Hydrogenated thiadiazines
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention is a kind of process for preparing high-content Bentazon sodium salt raw medicine and thus obtained Bentazon sodium salt solid, includes the following steps: a, prepares: solvent and Bentazon raw medicine being added in the reactor；B, it prepares: solid base sodium hydroxide, temperature rising reflux and the water for separating generation is added in the reactor again, until anhydrous separate；C, finished product: being cooled to room temperature for reactor, filters, and the Bentazon sodium salt solid of high-content can be obtained in drying.The present invention can directly prepare the Bentazon sodium salt of solid, solves the demand for needing high-content Bentazon sodium salt raw medicine to do compound product, packaging and transportation cost are not only reduced, improves economic results in society, and content is high, suitable for industrialized production, it can be directly dissolved in i.e. sprayable in water, or directly be compounded with other pesticides, greatly facilitate the operation and subsequent processing of peasant, multi-step processing is not needed again not only, more avoids the discharge of waste water.
Description
Technical field:
The present invention relates to herbicide field, in particular to a kind of process for preparing high-content Bentazon sodium salt raw medicine and
Thus obtained Bentazon sodium salt raw medicine.
Background technique:
Bentazon is a kind of broad spectrum activity killing type herbicide after seedling, be mainly used for soybean, wheat, rice, peanut, etc. make
Object prevents and kill off broadleaf weeds and sedge weed.Solubility is very small in water for Bentazon, and usual Bentazon formulation products are them
Sodium salt aqua, natrium brine agent content cannot be too high, not so have crystal precipitation, and the aqua of low concentration increases packaging and fortune
Defeated cost.Now there is an urgent need to provide a kind of technique to prepare Bentazon sodium salt solid raw medicine, first is that can greatly reduce in this way
Packaging and transportation cost, improve economic benefit；Second is that many agriculture chemical compounding products need the Bentazon sodium salt raw medicine of solid.
Trial Bentazon prepares the Bentazon sodium salt of solid with liquid caustic soda, and reaction is that Bentazon sodium can be generated in itself
Salt, but solid product cannot be precipitated after reaction, solid can not be precipitated with other solvent crystallizations after normal pressure or negative pressure dehydration
Shape product, while also bringing a large amount of waste water and needing to handle.Currently, also former without high-content Bentazon sodium salt solid both at home and abroad
The relevant report of medicament preparation.
Summary of the invention:
The purpose of the present invention is to the deficiencies of the prior art, and provide and a kind of prepare high-content Bentazon sodium salt raw medicine
Process and thus obtained Bentazon sodium salt raw medicine, the aqua of very good solution Bentazon low concentration increases packaging
And transportation cost, and liquid Bentazon is cumbersome when preparing compound product, generally requires multi-step processing, and bring
A large amount of waste water needs the problems such as handling.
Technical scheme is as follows:
The process for preparing high-content Bentazon sodium salt raw medicine, includes the following steps:
A, prepare: solvent and Bentazon raw medicine being added in the reactor；
B, it prepares: solid base sodium hydroxide, temperature rising reflux and the water for separating generation is added in the reactor again, until anhydrous
Until separating；
C, finished product: being cooled to room temperature for reactor, filters, and the Bentazon sodium salt solid of high-content can be obtained in drying.This
Sample can directly prepare the Bentazon sodium salt of solid, solve and high-content Bentazon sodium salt raw medicine is needed to do compound product
Demand not only reduces packaging and transportation cost, improves economic results in society, and content is high, is suitable for industrialized production, can
It is i.e. sprayable to be directly dissolved in water, or directly compounded with other pesticides, the operation of peasant is greatly facilitated with after
Continuous processing does not need again multi-step processing not only, this process is simple, at low cost, more avoids the discharge of waste water.
Preferably, solvent is organic solvent.
Preferably, solvent is toluene or dichloroethanes.
Preferably, solvent is toluene.Selection toluene is solvent, and not only cost is relatively low, but also good in compatibility, Ke Yiyou
The dissolution Bentazon raw medicine and solid base sodium hydroxide of effect can also be reused after reheating reflux, be further avoided useless
The discharge of water exhaust gas.
Preferably, solvent and the mass ratio of Bentazon raw medicine are 1.5~3:1 in preparation process.
Preferably, in preparation step Bentazon raw medicine and sodium hydroxide 1~1.3:1 of molar ratio.
Preferably, Bentazon raw medicine and the molar ratio of sodium hydroxide are 1.05:1 in preparation step.
Preferably, warming temperature is 84 DEG C~110 DEG C in preparation step.
The content of Bentazon sodium salt is 97%~99% in Bentazon sodium salt sodium salt solid raw medicine.This hair can thus be made
Packing and selling after bright Bentazon sodium salt sodium salt solid raw medicine obtained can be weighed directly, peasant can directly add water when in use
Or compounded with other kinds of liquid pesticidal, the use of peasant is greatly facilitated, the blank of related pesticide has been filled up, and
And cost is relatively low by the present invention, also improves the enthusiasm of peasant, ensure that the income of peasant.
The beneficial effects of the present invention are:
The present invention thus can directly prepare the Bentazon sodium salt of solid, solve and need high-content Bentazon sodium salt
Raw medicine does the demand of compound product, not only reduces packaging and transportation cost, improves economic results in society, and content is high, fits
It for industrialized production, can be directly dissolved in i.e. sprayable in water, or directly be compounded, greatly facilitated with other pesticides
The operation and subsequent processing of peasant does not need again multi-step processing not only, this process is simple, at low cost, more avoids
The discharge of waste water.
Specific embodiment:
Embodiment 1
200 g toluene and 100g Bentazon raw medicine (commercially available raw medicine, content 96%) are added in 500ml reaction flask, then plus
Enter 15.8 g(content 96% of solid sodium hydroxide), stirring is warming up to 96 DEG C of back flow reactions, the waterside reflux generated in reaction process
While separate to obtain mother liquor toluene A, until anhydrous separate, after be cooled to room temperature, filter, drying obtains Bentazon sodium salt
Solid 101.3g, content 98.5% filter mother liquid obtained toluene A set for lower batch of preparation.
Embodiment 2
The mother liquor toluene A in embodiment 1 is added in 500ml reaction flask, inadequate complements to 200 g with fresh toluene,
100 g Bentazon raw medicines (commercially available raw medicine, content 96%) are added, 16 g(content 96% of solid sodium hydroxide is then added), it stirs
It mixes and is warming up to 84 DEG C of back flow reactions, the waterside reflux side generated in reaction process, which separates out, obtains mother liquor toluene B, until no moisture
Until out, after be cooled to room temperature, filter, drying obtains Bentazon sodium salt solid 104.5g, content 98%, filtering gained
Mother liquor toluene B set is for lower batch of preparation.
Embodiment 3
Above-mentioned mother liquor toluene B is added in 1000ml reaction flask, inadequate complements to 400 g with fresh toluene, adds
32 g(content 96% of solid sodium hydroxide is then added in 200 g Bentazon raw medicines (commercially available raw medicine, content 96%)), stirring heating
To 110 DEG C of back flow reactions, the waterside reflux side generated in reaction process separates mother liquor toluene C, until anhydrous separate, terminates
After be cooled to room temperature, filter, drying obtain 203.6 g of Bentazon sodium salt solid, content 97.9% filters mother liquid obtained toluene C
Set is for lower batch of preparation.
Embodiment 4
Above-mentioned mother liquor toluene C is added in 1000ml reaction flask, inadequate complements to 400 g with fresh toluene, adds
34 g(content 96% of solid sodium hydroxide is then added in 200 g Bentazon raw medicines (commercially available raw medicine, content 96%)), stirring heating
To 105 DEG C of back flow reactions, the waterside reflux side generated in reaction process separates mother liquor toluene D, until anhydrous separate, terminates
After be cooled to room temperature, filter, drying obtain 208.6 g of Bentazon sodium salt solid, content 97.6% filters mother liquid obtained toluene D
Set is for lower batch of preparation.
The foregoing is merely presently preferred embodiments of the present invention, and those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, should fall within the scope of the present invention.
Claims (2)
1. preparing the process of Bentazon sodium salt raw medicine, characterized by the following steps:
A, prepare: solvent and Bentazon raw medicine being added in the reactor；
B, it prepares: solid base sodium hydroxide, temperature rising reflux and the water for separating generation is added in the reactor again, is separated until anhydrous
Until；
C, finished product: being cooled to room temperature for reactor, filters, and the Bentazon sodium salt solid of high-content can be obtained in drying；
Warming temperature is 84 DEG C~110 DEG C in the preparation step；
The solvent is toluene；
Solvent and the mass ratio of Bentazon raw medicine are 1.5~3:1 in the preparation process；
1~1.3:1 of molar ratio of Bentazon raw medicine and sodium hydroxide in the preparation step.
2. the process according to claim 1 for preparing Bentazon sodium salt raw medicine, it is characterised in that: the preparation step
Middle Bentazon raw medicine and the molar ratio of sodium hydroxide are 1.05:1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004146.4A CN105566249B (en) | 2015-12-29 | 2015-12-29 | Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004146.4A CN105566249B (en) | 2015-12-29 | 2015-12-29 | Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine |
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| Publication Number | Publication Date |
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| CN105566249A CN105566249A (en) | 2016-05-11 |
| CN105566249B true CN105566249B (en) | 2019-06-04 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5266553A (en) * | 1991-10-21 | 1993-11-30 | Riverdale Chemical Company | Method of manufacturing a dry water-soluble herbicidal salt composition |
| US5883047A (en) * | 1996-04-03 | 1999-03-16 | Basf Aktiengesellschaft | Granules of hygroscopic, water-soluble products |
| CN101481361A (en) * | 2008-01-09 | 2009-07-15 | 苏州联合伟业科技有限公司 | Technique of preparing high-purity bentazone raw pesticide |
| CN102617511A (en) * | 2012-03-09 | 2012-08-01 | 东北大学 | Wastewater-free preparation method of bentazon |
| CN102924404A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone sodium salt powder |
| CN104478829A (en) * | 2014-11-12 | 2015-04-01 | 浙江中山化工集团股份有限公司 | Preparation method of bentazone dimethylamine salt raw drug |
-
2015
- 2015-12-29 CN CN201511004146.4A patent/CN105566249B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5266553A (en) * | 1991-10-21 | 1993-11-30 | Riverdale Chemical Company | Method of manufacturing a dry water-soluble herbicidal salt composition |
| US5883047A (en) * | 1996-04-03 | 1999-03-16 | Basf Aktiengesellschaft | Granules of hygroscopic, water-soluble products |
| CN101481361A (en) * | 2008-01-09 | 2009-07-15 | 苏州联合伟业科技有限公司 | Technique of preparing high-purity bentazone raw pesticide |
| CN102617511A (en) * | 2012-03-09 | 2012-08-01 | 东北大学 | Wastewater-free preparation method of bentazon |
| CN102924404A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone sodium salt powder |
| CN104478829A (en) * | 2014-11-12 | 2015-04-01 | 浙江中山化工集团股份有限公司 | Preparation method of bentazone dimethylamine salt raw drug |
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| CN105566249A (en) | 2016-05-11 |
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